CN110015887A - 一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体及其制备方法 - Google Patents

一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体及其制备方法 Download PDF

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CN110015887A
CN110015887A CN201910256723.0A CN201910256723A CN110015887A CN 110015887 A CN110015887 A CN 110015887A CN 201910256723 A CN201910256723 A CN 201910256723A CN 110015887 A CN110015887 A CN 110015887A
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salt
powder
titanium
yttrium
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陈超
陈家荣
莫培程
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China Nonferrous Metal Guilin Geology and Mining Co Ltd
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Priority to US16/837,001 priority patent/US11345638B2/en
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Abstract

本发明提供了一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体及其制备方法，属于陶瓷材料技术领域，本发明提供的制备方法包括以下步骤：将铝盐、锆盐、钇盐、钛盐与水混合，得到混合水溶液；所述铝盐、锆盐、钇盐和钛盐为水溶性无机盐；将得到的混合水溶液与碱性沉淀剂混合进行沉淀，得到氢氧化物沉淀粉体；将得到的氢氧化物沉淀粉体依次进行第一煅烧和第二煅烧，得到氧化物固溶体粉体；将所得到的氧化物固溶体粉体选择性氮化反应，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。本发明提供的氮化钛补强氧化锆增韧氧化铝陶瓷粉体热压烧结得到的陶瓷材料硬度高，导电性能好。

Description

一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体及其制备方法
技术领域
本发明涉及陶瓷材料技术领域，特别涉及一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体及其制备方法。
背景技术
材料的力学、电学、光学等使用性能不仅取决于材料中各个组分的本身性质，还与材料组分之间的宏观层次和显微层次的结构密切相关。近年来，先进陶瓷材料的制备技术正朝着加更精细和微观可控的方向发展，强调陶瓷材料分子、原子尺度的复合和以固溶为基础的材料制备。在先进陶瓷材料研究中，与固溶体系相关的材料制备和材料改性技术，包括固溶强化、固溶掺杂、固溶分相、固溶体选择性反应等，是进行显微结构设计的重要方法。
氧化锆增韧氧化铝陶瓷材料(zirconia-toughenedalumina，ZTA)具有良好的力学性能，它的强度和韧性值可以通过调节Y2O3的掺杂量来调节，它的晶粒尺寸的大小控制、抑制相转变、促进材料的致密化可以通过Al2O3的含量来调节。但是硬度不高和导电性差限制了它的应用场合。
发明内容
有鉴于此，本发明目的在于提供一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体及其制备方法，本发明提供的氮化钛补强氧化锆增韧氧化铝陶瓷粉体经热压烧结得到的陶瓷材料硬度高，导电性好。
本发明提供一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体的制备方法，包括以下步骤：
1)将铝盐、锆盐、钇盐、钛盐与水混合，得到混合水溶液；所述铝盐、锆盐、钇盐和钛盐为水溶性无机盐；
2)将所述步骤1)得到的混合水溶液与碱性沉淀剂混合进行沉淀，得到氢氧化物沉淀粉体；
3)将所述步骤2)得到的氢氧化物沉淀粉体依次进行第一煅烧和第二煅烧，得到氧化物固溶体粉体；所述第一煅烧的温度为700～850℃，时间为6～12h；第二煅烧的温度为900～1000℃，时间为1～3h；
4)将所述步骤3)得到的氧化物固溶体粉体进行选择性氮化反应，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
优选地，所述步骤1)中铝盐包括氯化铝、硫酸铝或硝酸铝；锆盐包括氯氧化锆或柠檬酸锆；钇盐包括氯化钇、硝酸钇或硫酸钇；钛盐包括硫酸钛、氯化钛或硝酸钛。
优选地，所述步骤1)中铝盐中的铝、锆盐中的锆、钇盐中的钇和钛盐中的钛的摩尔比为(10～30)：(30～70)：(0.4～1)：(5～20)。
优选地，所述步骤2)中碱性沉淀剂为氨水或氯化铵。
优选地，所述步骤2)中沉淀后还包括对所得体系固液分离，对固液分离所得固体进行干燥，得到氢氧化物沉淀粉体。
优选地，所述干燥的温度为75～85℃。
优选地，所述步骤4)中选择性氮化反应的温度为800～1200℃。
本发明还提供了上述制备方法制备得到的氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
有益技术效果：本发明提供了一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体及其制备方法，包括以下步骤：将铝盐、锆盐、钇盐、钛盐与水混合，得到混合水溶液；所述铝盐、锆盐、钇盐和钛盐为水溶性无机盐；将得到的混合水溶液与碱性沉淀剂混合进行沉淀，得到氢氧化物沉淀粉体；将得到的氢氧化物沉淀粉体依次进行第一煅烧和第二煅烧，得到氧化物固溶体粉体；所述第一煅烧的温度为700～850℃，时间为6～12h；所述第二煅烧的温度为900～1000℃，时间为1～3h；将所得到的氧化物固溶体粉体选择性氮化反应，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。本发明将氮化钛引入氧化锆增韧氧化铝陶瓷材料，一方面利用氮化钛的高熔点、高硬度来提高氧化锆增韧氧化铝陶瓷材料的耐磨性能和硬度，并起到补强增韧的效果；另一方面，利用氮化钛的高导电性，增强陶瓷粉体的导电性。本发明并未直接将氮化钛粉体与氧化锆增韧氧化铝陶瓷粉体机械混合后在进行烧结，而是在分子水平进行混合并通过煅烧得到氧化物，并通过选择性氮化原位合成氮化钛补强氧化锆增韧氧化铝陶瓷粉体，可以有效地降低复相材料中显微结构的不均匀性，改善第二相与基体的物理化学相容性，提高材料的热稳定性。
附图说明：
图1为实施例1中得到的氮化钛补强氧化锆增韧氧化铝陶瓷粉体的X射线衍射图谱。
具体实施方式
本发明提供了一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体的制备方法，包括以下步骤：
1)将铝盐、锆盐、钇盐、钛盐与水混合，得到混合水溶液；所述铝盐、锆盐、钇盐和钛盐为水溶性无机盐；
2)将所述步骤1)得到的混合水溶液与碱性沉淀剂混合进行沉淀，得到氢氧化物沉淀粉体；
3)将所述步骤2)得到的氢氧化物沉淀粉体依次进行第一煅烧和第二煅烧，得到氧化物固溶体粉体；所述第一煅烧的温度为700～850℃，时间为6～12h；第二煅烧的温度为900～1000℃，时间为1～3h；
4)将所述步骤3)得到的氧化物固溶体粉体进行选择性氮化反应，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
本发明将铝盐、锆盐、钇盐、钛盐与水混合，得到混合水溶液；所述铝盐、锆盐、钇盐和钛盐为水溶性无机盐。
在本发明中，所述铝盐优选包括氯化铝、硫酸铝或硝酸铝；锆盐优选包括氯氧化锆或柠檬酸锆；钇盐优选包括氯化钇、硝酸钇或硫酸钇；钛盐优选包括硫酸钛、氯化钛或硝酸钛。
在本发明中，所述铝盐中的铝、锆盐中的锆、钇盐中的钇和钛盐中的钛的摩尔比优选为(10～30)：(30～70)：(0.4～1)：(5～20)，更优选为(15～25)：(40～50)：(0.5～0.8)：(10～15)。
本发明对水的用量没有特殊限定，选用本领域技术人员熟知的用量，能够使铝盐、锆盐、钇盐和钛盐全部溶解即可。
本发明对混合的方法没有特殊限定，选用本领域技术人员熟知的混合方法即可。
得到混合水溶液后，本发明将混合水溶液与碱性沉淀剂混合进行沉淀，得到氢氧化物沉淀粉体。
在本发明中，所述碱性沉淀剂优选为氨水或氯化铵。本发明对所述碱性沉淀剂的用量没有特殊限定，能够使铝盐、锆盐、钇盐和钛盐中的阳离子沉淀完全即可。
本发明对混合水溶液与碱性沉淀剂混合的方法没有特殊限定，选用本领域技术人员熟知的混合方法即可。在本发明的一个实施例中，优选为搅拌混合，本发明对所述搅拌的速率和时间没有特殊限定，选用本领域技术人员熟知的搅拌速率和时间即可；在本发明中，所述混合的时间即为沉淀的时间。
在本发明中，所述沉淀后还优选包括对所得体系固液分离，对固液分离所得固体进行干燥，得到氢氧化物沉淀粉体。
在本发明中，所述氢氧化物沉淀粉体包括Al(OH)3、Zr(OH)2、Y2(OH)3和Ti(OH)2。
本发明对固液分离的方法没有特殊限定，选用本领域技术人员熟知的固液分离方法即可，如过滤。
在本发明中，所述干燥的温度优选为75～85℃。本发明对干燥的时间没有特殊限定，干燥至恒重即可。
在本发明中，所述干燥前还优选包括对固液分离后所的固体依次进行水洗和醇洗。本发明对水洗的方法没有特殊限定，选用本领域技术人员熟知的水洗方法即可；本发明通过水洗除去反应物中的杂质离子。在本发明中，所述醇洗优选为使用无水乙醇进行洗涤，本发明对使用无水乙醇进行洗涤的方法没有特殊限定，选用本领域技术人员熟知的洗涤方法即可。本发明通过醇洗脱除水分，消除胶粒之间借助水分子形成的桥氧键，避免煅烧过程中形成粉体的硬团聚。
得到氢氧化物沉淀粉体后，本发明将所述氢氧化物沉淀粉体依次进行第一煅烧和第二煅烧，得到氧化物固溶体粉体；所述第一煅烧的温度为700～850℃，时间为6～12h；所述第二煅烧的温度为900～1000℃，时间为1～3h。
在本发明中，所述第一煅烧的温度为700～850℃，优选为750～800℃；所述第一煅烧的时间为6～12h，更优选为8～10h。本发明优选从室温升温至第一煅烧温度进行煅烧。本发明对升温速率没有特殊限定，选用本领域技术人员熟知的升温速率即可。本发明通过第一煅烧使所述氢氧化物沉淀粉体中的Al(OH)3、Zr(OH)2、Y2(OH)3和Ti(OH)2转化为Al2O3、ZrO2、Y2O3和TiO2。
在本发明中，所述第二煅烧的温度为900～1000℃，更优选为950～980℃；所述第二煅烧的时间为1～3h，更优选为1.5～5h。本发明优选从第一煅烧温度升温至第二煅烧温度进行第二煅烧。本发明对升温速率没有特殊限定，选用本领域技术人员熟知的升温速率即可。本发明通过第二煅烧使Al2O3，ZrO2充分共同结晶，形成固溶体，Ti4+，Y3+离子完全进入氧化铝和氧化锆晶格中，同时Y2O3对四方氧化锆起稳定作用，从而获得氧化物固溶体粉体。在本发明中，所述氧化物固溶粉体粉体的粒径优选为10～25nm，更优选为15～20nm。
在本发明中，所述第一煅烧和第二煅烧优选在空气中进行。
得到氧化物固溶体粉体后，本发明优选将所述氧化物固溶体粉体进行选择性氮化反应，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
在本发明中，所述选择性氮化反应的温度优选为800～1200℃，更优选为900～1000℃。在本发明中，所述Al2O3、ZrO2、Y2O3与氮气的反应温度较高，均在1300℃以上，因此本发明通过控制选择性氮化反应的温度只使TiO2氮化。
在本发明中，所述选择性氮化反应的氮化试剂优选为氨气。本发明对进行选择性氮化反应的装置没有特殊限定，选用本领域技术人员熟知的装置即可。具体地，本发明将所述氧化物固溶体粉体放入氧化铝瓷舟中，将氧化铝瓷舟放入真空管式高温电炉中，通入流动的高纯氨气进行选择性氮化反应。
本发明还提供了上述制备方法制备得到的氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明的内容不仅仅局限于下面的实施例。
实施例1
在水中加入氯氧化锆(ZrOCl2·8H2O)、氯化铝(AlCl3)和氯化钇(YCl3)，硫酸钛(Ti(SO4)2)制备混合水溶液，氯化铝、氯氧化锆和硫酸钛的摩尔比为60：25：15，氯氧化锆与氯化钇的摩尔比为98.5：3。混合均匀后，添加氨水，充分搅拌沉淀，过滤，依次进行水洗和无水乙醇洗涤，烘干，得到氢氧化物沉淀粉体。将得到的氢氧化物沉淀粉体在空气中煅烧700℃保温9小时，进一步煅烧900℃保温1小时，从而获得氧化物固溶体粉体(Al2O3，ZrO2，Y2O3和TiO2)。将Al2O3-ZrO2-Y2O3-TiO2固溶体粉体放入99％的氧化铝瓷舟中，然后将氧化铝瓷舟放入真空管式高温电炉中，通入流动的高纯氨气，在高温下进行选择性氮化反应，反应温度在900℃，反应时间为5h，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
图1为实施例1中得到的氮化钛补强氧化锆增韧氧化铝陶瓷粉体的X射线衍射图谱。由图1可知，实施例1中得到的氮化钛补强氧化锆增韧氧化铝陶瓷粉体粒径约为94nm。
将实施例1得到的氧化铝陶瓷粉体热压烧结，所得陶瓷材料的硬度为25GPa，磨耗比为3000：1，具有导电性能。
实施例2
在水中加入氯氧化锆(ZrOCl2·8H2O)、硝酸铝(AlNO3)和硝酸钇(Y(No3)3)，硫酸钛(Ti(SO4)2)制备混合水溶液，氯氧化锆、硝酸铝和硫酸钛的摩尔比为60：25：15，氯氧化锆与氯化钇的摩尔比为97.5：3。混合均匀后，添加氨水，充分搅拌沉淀，过滤，依次进行水洗和无水乙醇洗涤，烘干，得到氢氧化物沉淀粉体。将得到的氢氧化物沉淀粉体在空气中煅烧700℃保温9小时，进一步煅烧900℃保温1小时，从而获得氧化物固溶体粉体(Al2O3，ZrO2，Y2O3和TiO2)。将Al2O3-ZrO2-Y2O3-TiO2固溶体粉体放入99％的氧化铝瓷舟中，然后将氧化铝瓷舟放入真空管式高温电炉中，通入流动的高纯氨气，在高温下进行选择性氮化反应，反应温度在900℃，反应时间为5h，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
将实施例2得到的氧化铝陶瓷粉体热压烧结，所得陶瓷材料的硬度为35GPa，磨耗比为6000：1，具有导电性能。
实施例3
在水中加入氯氧化锆(ZrOCl2·8H2O)、氯化铝(AlCl3)和氯化钇(YCl3)，硫酸钛(Ti(SO4)2)制备混合水溶液，氯氧化锆、氯化铝和硫酸钛的摩尔比为50：30：20，氯氧化锆与氯化钇的摩尔比为98.5：3。混合均匀后，添加氨水，充分搅拌沉淀，过滤，依次进行水洗和无水乙醇洗涤，烘干，得到氢氧化物沉淀粉体。将得到的氢氧化物沉淀粉体在空气中煅烧700℃保温9小时，进一步煅烧900℃保温1小时，从而获得氧化物固溶体粉体(Al2O3，ZrO2，Y2O3和TiO2)。将Al2O3-ZrO2-Y2O3-TiO2固溶体粉体放入99％的氧化铝瓷舟中，然后将氧化铝瓷舟放入真空管式高温电炉中，通入流动的高纯氨气，在高温下进行选择性氮化反应，反应温度在950℃，反应时间为1h，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
将实施例3得到的氧化铝陶瓷粉体热压烧结，所得陶瓷材料的硬度为30GPa，磨耗比为5000：1，具有导电性能。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (8)

1.一种氮化钛补强氧化锆增韧氧化铝陶瓷粉体的制备方法，包括以下步骤：
1)将铝盐、锆盐、钇盐、钛盐与水混合，得到混合水溶液；所述铝盐、锆盐、钇盐和钛盐为水溶性无机盐；
2)将所述步骤1)得到的混合水溶液与碱性沉淀剂混合进行沉淀，得到氢氧化物沉淀粉体；
3)将所述步骤2)得到的氢氧化物沉淀粉体依次进行第一煅烧和第二煅烧，得到氧化物固溶体粉体；所述第一煅烧的温度为700～850℃，时间为6～12h；所述第二煅烧的温度为900～1000℃，时间为1～3h；
4)将所述步骤3)得到的氧化物固溶体粉体进行选择性氮化反应，得到氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
2.根据权利要求1所述的制备方法，其特征在于，所述步骤1)中铝盐包括氯化铝、硫酸铝或硝酸铝；锆盐包括氯氧化锆或柠檬酸锆；钇盐包括氯化钇、硝酸钇或硫酸钇；钛盐包括硫酸钛、氯化钛或硝酸钛。
3.根据权利要求1或2所述的制备方法，其特征在于，所述步骤1)中铝盐中的铝、锆盐中的锆、钇盐中的钇和钛盐中的钛的摩尔比为(10～30)：(30～70)：(0.4～1)：(5～20)。
4.根据权利要求1所述的制备方法，其特征在于，所述步骤2)中碱性沉淀剂为氨水或氯化铵。
5.根据权利要求1所述的制备方法，其特征在于，所述步骤2)中沉淀后还包括对所得体系固液分离，对固液分离所得固体进行干燥，得到氢氧化物沉淀粉体。
6.根据权利要求5所述的制备方法，其特征在于，所述干燥的温度为75～85℃。
7.根据权利要求1所述的制备方法，其特征在于，所述步骤4)中选择性氮化反应的温度为800～1200℃。
8.权利要求1～7任意一项所述的制备方法制备得到的氮化钛补强氧化锆增韧氧化铝陶瓷粉体。
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